Lubrication composition



Patented Sept. 23, 1952 2,611,743 LUBRICATION COMRQSITION Egbert Mason Kipp, New Kensington, -Pa., 'assigner to inum Company .of America,

Pittsburgh, 2a., a corporation .o'f Pennsylvania .NofDrawing. ApplicationDecemberf1'Z,i1949,

' SerialTNo. 133; 682

This invention relates to improved lubricants, such as oils, greases or semi-fluid-oils, containing as a major lubricating component hydrocarbon oil of natural or synthetic origin. In particular, the invention relates to lubricating compositions of this type having improved extreme pressure characteristics.

Requirements uponlubricants"by-developments in mechanical-design "are rigid-and drastic. in many instances pressures-at bearingsur'faces-are higher than thosewhich petroleumoils will normally withstand. Illustrative are theconditions encountered in the lubrication of automotive hypoid gears, heavily loaded mill pinion gears, naval turret gears and the like. In many =machines operation is, at least in part, under conditions of thin film lubrication or under similar conditions where film strength, oiliness and anti-wear characteristics of high order 'are re-- quired of the lubricating medium.

The principal objector this invention is the provision of "a new composition of matter consistingof a compounded lubricatingproduct possessing extreme pressure characteristics of -a high order. "Further objects include 'the provision of a compounded lubricant containing as a major hydrocarbon'lubricating component which may be oil or grease of "natural or synthetic origin, the lubricant having -a superior combination of high film strength, oiliness-and anti-wear characteristics. v

In accordance with this invention these objects are achieved'in substantial part by Providing a lubricant, the essential lubricating com-- ponents of which area major amount of a hydrocarbon lubricating component which may be oil orgrease and a minor :amount of a boron fluoride fatty acid .body more specifically described below. The proportion of this :body to the;hydrocarbon componentshould be such, however, that .the mixture contains atleast 0.001 percent by weight of boron fluoride (BFs) while, on the other'hand, more-than ,3 percent does not improve thelubricant. Within thisrange'it has been found that the best results are obtainedby providing from 0.1 .to 1.0;percent of boron fluoride in the final lubricant mixture. The choice of the particular body .to be employed and its boron fluoride content will, of course, depend on such matters as cost, ease of mixing and the nature of the lubrication problem.

The principal advantages and'efiectiveness of this new compoundedzlubricant are maintained nclaims. r(c1. zsz iac) 2 when, in addition :to the above .:mentioned essential components there are likewise -,presen t in ithel lubricating composition other componentsadded to improvesome specific characteristic-pr property thereof; such .as viscosity, pour zpoint, pills. ness, flow, anti-wear characteristics, film strength or the like, the 'efiectnf "the defined boron :fiuo.-

rideecontainingibody, 'whenzsimilar, being largely additive. :Suchdiluents oradditions.'may;theree fore, forxthe .purposes .of ithlS :inventiont-be re:

garded as a non-essential :portionipf :the 560111130:

sition, regardless of their specific beneficial-sot;

functional efiect. 'Thessame.mayabe-saidrofzsubstances :known .as .extreme .zpressure :additives;

boron rfiuorideecontaining bodies is gefiectivp cto increase the extreme :pressure ,characteristics =01 the compositions seven when :other extreme press sure additives are present.

The organic JBFs b ody,;.which with this invention ;is' blended -1Withi-fihe hydro! carbon component, :may the. prepared zin ryarious.

ways abut gis, :ior the most part, convenientlyprepared by exposing the fatty acid ito directrconr;

tact with gaseous ,;BF3.. This ccan Joev easilyvv fies) complished under ordinary atmosphericpr essure by :bubbling :the gaseous 1BR; through :the :iattyacid;;in :a:liquid state. If .the :iatty acid :is' not liquid "at ;room .ltemperature it should 'be :heated;

to and maintained at a temperature slightly?- above itsmelting pointysayh or:10?.;C Although,

themateioif; flow of thegasismot critical .with :re.- spect :to theiormatioaoi 1thevsBFaadditive yet the. flew. should; becontrolled:tdavoidnndueloss;

The :r ate of ;ac.cep.tance -;oi the :BE; :by -the fatty a id; is wimprovejdrif the liquid is:=stirr ed;as thergas:

is introduced. The amount 013E: .accepted Jay the ,-iatty acid .:is indicated :by :the increase 1-inweight-of it-heitreatedmass. :The; introductionoi the gas may .thereforeibe continued: until .al redetermined increase in weight, short of .saturation, hasbeenobtained or the flow-of. gas may'ibe prolonged .untikno inrth er increase in aweight-iisi s ed t which po n the fatty :acid: isz'com-I sidered t0 the saturated with 3135's.. :Generallypit is most convenient .to: follow ;the;latter: rocedure; In =,both, cases, however, :the :length of .-.;time res: qu red to reach :;the. endpoint pan the easilyrdeeiz termined @or the .ifatty .acid being treated :and hus .-.-make::it possible, 300 zintroducezthexdesired imQll t1 i1BFa without hailingeto' test a charge? t nt rva:1s durin -ithe :period of :ireatmenta in -:accordancet 3 Although each fatty acid may have a different saturation point or the desired BFs content may differ for various fatty acids this does not detract from the value of the BFa-containing body in improving the load bearing quality of a hydrocarbon lubricant.

Other methods of introducing BFs can be employed, of course. For example, the fatty acid may be exposed to the gas at higher temperatures and pressures and thus shorten the time required to introduce the desired amount of BFs. Natu-.

rally, the temperature and pressure should be such that the fatty acid is not decomposed'to any substantial degree. Another method of contacting the fatty acid with BFs is to add compounds to the fatty acid which can be decom posed with the release of BFs. Such compounds cant and, in many instances, to definitely imas NH4BF4, BFs-NHa, the heavy metal fluoborates' or even other organic materials: previously treated with BFs may be employed. To effect decomposi-- tion it is usually necessary to heat the mixture of fatty acid and the BFa-containing substance.- Further, it may be desirable to remove any residues .resulting from the decomposition.

The amount of BF3 that can be introduced into different fatty acids will vary, as mentioned above, however, from 10 to percent by weight is preferred where the saturation point permits it. In any case, the fatty acids should be treated with suflicient fluoride to provide the desired BF: content in the lubricating composition as only a minor proportion of the additive is employed.

- The resultant product may, in some instances, bean actual compound, there being some evidence to indicate that such isits nature, or it may be an additive or coordinate compound or even a solution or dispersion. I prefer, however, to term the product a body or composition consisting essentially of fatty acid and BFs and, therefore not to characterize the stateof association of the fluoride and the fatty. acid. In anyevent, the fatty acids act as acceptors of BF: to produce a body or substance having positive advantages as an additive in lubricating compositions.

The following list of fatty acids is illustrative of the class which when treated with BFa produce the bodies just described: normal straight chain saturated fatty. acids such as 'butyric, caproic, caprylic, capric,lauric, myristic, palmitic, stearic and arachidic; intermediate odd numbered acids such as pentanoic, heptanoic through heptadecanoic; monoethylenic acids such as pentenoic, hexenoic, heptenoic through oleic; dienoic acids such as linoleic; trienoic acids such as linolenic; hydroxy acids such as hydroxy hexanoic through ricinoleic; keto fatty acids such as the straight chain alkyl carboxylic acids containing one or more carbonyl groups in the hydrocarbon portion of the molecule as illustrated by keto valeric through keto octadecanoic; cyclic acids such as chalumoorgic, and saturated dicarboxylic such as ethanedioic through heneicosanedioic and nonadecamethylene 1,19-dicarboxylic acid.

The introduction of the BF: into the fatty acid may change the color of the fatty acid, often making it darker. Also, the liquid fatty acid may become thicker as the introduction of BFs proceeds and the melting point of the end product may be higher than that of the original fatty acid. Such changes do not affect the advantages gained from the presence of the BEE-containing bodies in a hydrocarbon lubricant, certainly the results of the invention do not depend upon or are responsive to any peculiar chemical or physiprove its-anti-wear characteristics; The amount of these organic BF3 bodies .necessarily present to produce these specific effects is very small. The amounts used, should in any case, as mentioned above, provide at least 0.001 percent by weight of BFa in the final mixture. The amount of any given El 's-containing body desirably present toproduce optimum efiects in any particular hydrocarbon lubricant can be readily determined by simple trial, the optimum usually being found within the rangeof 0.5 to 5 percent by weight of the fatty acid BF: body. Amounts below about 0.01 percent by weight often do not produce sufficient effect to be usually characterized as commerciai, but the effect produced is such as to be useful under exceptional conditions. One may use a relatively small amount of an additive containing a substantial quantity of BF: or a larger amount of the same oranother additive which contains a smaller proportion of BFs to introduce a given quantity of BFc into the hydrocarbon component. In any event, the organic BFb additive forms a minoramountor proportion. of the I lubricatin composition.

. The load bearing qualities ofa lubricant may be relatively determinedby various methods. The method used to obtainthe comparative data hereinafter set forth is practiced on a Falex machine and consists in submitting-small quantities of the lubricant to the action ofja rotating steel journal rotated in contact with two V shaped bearing blocks. Duringt esting measurable pressure was applied to the rotatingjournal by use of an auto-, matic loading device. The two bearing blocks and the journal were submerged in the lubricant sample throughout the tests. In each test load was applied and allowed to reach 500 pounds; at this load the journal wasthen run for 5 minutes; thereafter theload was gradually increased until lubrication failure occurred. The load at the time of failure is designated vas the failure load. In general, the failure loads are reproducible within 150 pounds at lower pressure and 300 pounds at higher pressure; the results are not absolute but are comparative with astandard run under the same conditions. Inthe tests by which the results set forth in. the following table were secured, the hydrocarbon oil was in allcases the same, being a straight mineral oil. In all cases 1 percent by weight of additive was present in the fatty acid became saturated with the 31%, as has been described hereinabove. Each comparative test was run on two samples, one sample being the oil containing 1 percent by weight of a'fatty acid, the other sample being; the 011- containing the same weightof a BFi-containing body. In the firstcolumn of the tablethe nature of theadditive is set forth, in the second column is listed the BF: content of the treated material, in the third column is the BFs-content of the lubricant, in the fourth column the failure load in pounds is given and in-the fifth column is shown the percentage increase in failure load caused by the presence of the El 's-containing bodyfl 5 Percent Percent Failure Percent- Additive BF: in B F; in Load in age Additive Lubricant Pounds Increase Stearic acid 1, 100 I 260 Stearic acid+BFa- 18 0. 18 1 4, 000 Oleic acid 950 1 320 Oleic acid-i-IBFa 16 0. l6 1 4,000 Laurie acid 800 37o Laurie acid+B F3. 25 0. 25 3, 750 Oaproic acid 630 530 Caproic acid+B Fa 38 0. 38 3, 950 Ricinoleic acid 800 1 400 Ricinoleic acid+B F3. 9 0. 09 1 4, 000 Linoleic acid 9S0 220 Linoleic acid-i-BFa. 11. 4 0. 11 3, 100

1 Greater than.

The machine on which the tests were run had a capacity of 4500 pounds. Where this capacity was approximated or exceeded the failure load is indicated above as being greater than 4000 pounds. These tabulated results are indicative of the improvement obtained by the practice of this invention. In general, torque and temperature values obtained during these tests indicated that the organic BFa body improved friction qualities and observations simultaneously made indicated increases in anti-wear characteristics.

In compounding lubricant compositions of the type herein described and claimed the organic BFs additive may merely be mixed with the hydrocarbon lubricants, the properties of which are to be improved. Where the additive is insoluble in the lubricant or it is desired to incorporate therein amounts in excess of solubility, emulsions or dispersions may be prepared according to known principles,

This application is a continuation-in-part of my prior application Serial No. 714,908 filed December 7, 1946, now abandoned, and entitled Lubrication Composition.

Having thus described my invention and the known advantages thereof, I claim:

1. A lubricating composition comprising a major proportion of a hydrocarbon lubricating oil blended with a minor proportion of a body consisting essentially of fatty acid containing from 4 to 21 carbon atoms and BFb, said body being prepared by exposing the fatty acid to direct contact with a substance selected from the group composed of gaseous BF3 and decomposable compounds yielding gaseous BF: and being present in such amount thatthe lubricating composition contains from 0.001 to 3 per cent by weight of BF: said lubricating composition possessing extreme pressure characteristics superior to those exhibited by a similar composition in which the minor proportion aforesaid consists of fatty acid.

2. A lubricating composition comprising a major proportion of a hydrocarbon lubricating oil blended with a minor proportion of a body consisting essentially of stearic acid and BFs, said body being prepared by exposing the stearic acid to direct contact with a substance selected from the group composed of gaseous BFa'and decomposable compounds yielding gaseous BF: and being present in such amount that the lubricating composition contains from 0.001 to 3 per cent by weight of BFa said lubricating composition possessing extreme pressure characteristics superior to those exhibited by a similar composition in which the minor proportion aforesaid consists of stearic acid.

3. A lubricating composition comprising a major proportion of a hydrocarbon lubricating oil blended with a minor proportion of abody consisting essentially of oleic acid and BFa, said body being prepared by exposing the oleic acid to direct contact with a substance selected from the group composed of gaseous BFs and decomposable compounds yielding gaseous BF'zi and being present in such amount that the lubricating composition contains from 0.001 to 3 per cent by weight of BFs said lubricating composition possessing extreme pressure characteristics superior to those exhibited by a similar composition in which the minor proportion aforesaid consists of oleic acid.

4. A lubricating composition comprising a major proportion of a hydrocarbon lubricating oil blended with a minor proportion of a body consisting essentially of ricinoleic acidandBFb, said body being prepared by exposing the ricinoleic acid to direct contact with a substance selected from the group composed of gaseous BFs and de composable compounds yielding gaseous BF; and being present in such amount that the lubricating compositioncontains from 0.001 to 3 per cent by weight of BFa said lubricating composition possessing extreme pressure characteristics superior to those exhibited by a similar composition in which the minor proportion aforesaid consists of ricinoleic acid.

EGBERT MASON KIPP.

REFERENCES CITED The following references are of record in the file of this patent:

UNITED STATES PATENTS Number Name Date 2,053,474 Graves Sept. 8, 1936 2,160,917 Shoemaker June 6, 1939 2,266,060 Miller Dec. 16, 1941 FOREIGN PATENTS Number Country Date 645,202 Great Britain Jan. 9, 1948 645,425 Great Britain Jan. 9, 1948 OTHER REFERENCES "Boron Triiiuoride and Its Derivatives," Booth et al., John Wiley 8: Sons, 1949, pp. 64-67. 

1. A LUBRICATING COMPOSITION COMPRISING A MAJOR PROPORTION OF A HYDROCARBON LUBRICATING OIL BLENDED WITH A MINOR PROPORTION OF A BODY CONSISTING ESSENTIALLY OF FATTY ACID CONTAINING FROM 4 TO 21 CARBON ATOMS AND BF3, SAID BODY BEING PREPARED BY EXPOSING THE FATTY ACID TO DIRECT CONTACT WITH A SUBSTANCE SELECTED FROM THE GROUP COMPOSED OF GASEOUS BF3 AND DECOMPOSABLE COMPOUNDS YIELDING GASEOUS BF3 AND BEING PRESENT IN SUCH AMOUNT THAT THE LUBRICATING COMPOSITION CONTAINS FROM 0.001 TO 3 PER CENT BY WEIGHT OF BF3 SAID LUBRICATING COMPOSITION POSSESSING EXTREME PRESSURE CHARACTERISTICS SUPERIOR OF THOSE EXHIBITED BY A SIMILAR COMPOSITION IN WHICH THE MINOR PROPORTION AFORESAID CONSISTS OF FATTY ACID. 